CN107699958A - A kind of manufacture craft of mulberry silk - Google Patents

A kind of manufacture craft of mulberry silk Download PDF

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Publication number
CN107699958A
CN107699958A CN201710904004.6A CN201710904004A CN107699958A CN 107699958 A CN107699958 A CN 107699958A CN 201710904004 A CN201710904004 A CN 201710904004A CN 107699958 A CN107699958 A CN 107699958A
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Prior art keywords
silk
temperature
liquid
cocoon
water
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Inventor
兰建勇
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YIZHOU ZHUANGGE SILK Co Ltd
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YIZHOU ZHUANGGE SILK Co Ltd
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Priority to CN201710904004.6A priority Critical patent/CN107699958A/en
Publication of CN107699958A publication Critical patent/CN107699958A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01BMECHANICAL TREATMENT OF NATURAL FIBROUS OR FILAMENTARY MATERIAL TO OBTAIN FIBRES OF FILAMENTS, e.g. FOR SPINNING
    • D01B7/00Obtaining silk fibres or filaments
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B13/00Treatment of textile materials with liquids, gases or vapours with aid of vibration
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/04Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of yarns, threads or filaments
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06LDRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
    • D06L1/00Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
    • D06L1/12Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using aqueous solvents
    • D06L1/16Multi-step processes
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    • D06LDRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
    • D06L4/00Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
    • D06L4/10Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen
    • D06L4/12Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen combined with specific additives
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    • D06LDRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
    • D06L4/00Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
    • D06L4/10Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen
    • D06L4/13Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen using inorganic agents
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    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/02Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
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    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/48Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
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    • D06M11/73Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/76Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
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    • D06M11/77Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
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    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46Compounds containing quaternary nitrogen atoms
    • D06M13/463Compounds containing quaternary nitrogen atoms derived from monoamines
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    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/285Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
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    • D06M15/564Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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  • Engineering & Computer Science (AREA)
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  • Physics & Mathematics (AREA)
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  • Materials Engineering (AREA)
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  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
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  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The present invention provides a kind of manufacture craft of mulberry silk, belongs to textile technology field.Comprise the following steps:Refrigeration, vacuum infiltration, filature, refining, it is expanded, washing and it is flame-retardant modified.Wherein refining includes:Pretreatment, just practice, white silk, bleaching and cleaning again.The manufacture craft of the mulberry silk, after silk cocoon is refrigerated, the freshness of silkworm chrysalis being kept, by fresh silk cocoon directly by can directly be reeled off raw silk from cocoons after vacuum infiltration, reducing drying, cocoon cooking link, saving of labor, time saving, energy-conservation.And handled by refining, expanded and fire retardant, lift the flexibility, elasticity and anti-flammability of mulberry silk.

Description

A kind of manufacture craft of mulberry silk
Technical field
The present invention relates to textile technology field, a kind of specific manufacture craft of mulberry silk.
Background technology
Mulberry silk is one of animal origin that the mankind utilize earliest, because mulberry silk is from planting mulberry and breeding silkworm to the life of filature knit silk fabric Pollution is not affected by during production, therefore is the green product that the world is praised highly.Again because it is protein fibre, genus polyporus material, Good permeability, hygroscopicity is splendid, and is described as " fiber queen " by common people.Mulberry silk is as textile raw material, and the fabric being made into is not Only soft personal, heat-insulation breathable, also because of its green and healthy characteristic, has various health-care to human body.So mulberry silk is One of outstanding fiber of high-grade fabric is made.
Mulberry silk is silk liquid in silkworm body concretionary fiber, referred to as silk after spinning spues.It is transversal by two Face forms in the fibroin of nearly triangle or half elliptic (also known as fibroin) outsourcing silk gum, also pigment, oily wax and inorganic matter, they It is present in silk gum.Wherein silk gum has certain protective effect to fibroin, but if content is excessive, influences whether the gloss of fibroin Processed with the technique of sense and silk fiber, and the impurity such as grease, wax can bring certain difficulty to post-processing.Therefore, contaminating Before whole processing, it is necessary to first remove the debris such as most of silk gum, grease, wax, make silk fiber soft, loose, clean.
The preparation method of existing mulberry silk mainly comprises the following steps:(1) using the silk cocoon after cocoon drying as raw material, by it Silk floss sheet is made after being sprayed with alkaline spray liquid (such as solution containing sodium hydroxide) in silk floss machine in blanking;(2) by above-mentioned silk Continuous piece carries out refining degumming;(3) made through washing, final finishing, dehydration, drying.However, there are the following problems for the above method:Need Fresh cocoon is subjected to cocoon drying operation, adds production link, it is relative to improve production cost;In having carried out cocoon drying operation, obtain Silk cocoon in silk gum be denatured, that is, be transformed to indissoluble silk gum, therefore be required in spraying and refining scouring processes Alkali lye is used, this not only adds technology difficulty, and reduces the flexibility of silk mulberry.In addition, annual output cocoon batch is more at present, go out Cocoon is early, possesses abundant fresh cocoon resource.Therefore, how using the fresh cocoon resource in this part, directly silkworm is made by raw material of fresh cocoon Silk, it is a problem of the pendulum in face of technician.
The content of the invention
The goal of the invention of the present invention is, in view of the above-mentioned problems, providing a kind of manufacture craft of mulberry silk, silk cocoon to be carried out cold Behind Tibetan, keep the freshness of silkworm chrysalis, by fresh silk cocoon directly by can directly be reeled off raw silk from cocoons after vacuum infiltration, reduce drying, Cocoon cooking link, saving of labor, time saving, energy-conservation.And by refining, the processing of expanded and fire retardant, lifted the flexibility of mulberry silk, elasticity and Flame retardant effect.
To reach above-mentioned purpose, the technical solution adopted in the present invention is:
A kind of manufacture craft of mulberry silk, comprises the following steps:
S1. refrigerate:The fresh silkworm cocoon freezing of butterfly is not changed pupa but, cryogenic temperature is controlled at -20~-15 DEG C, soon Speed kills fresh silkworm cocoon, and then temperature is slowly warming up to -10~-5 DEG C of preservations, keeps the freshness of fresh silkworm cocoon.
S2. vacuum infiltration:The method of silk cocoon vacuum infiltration after refrigeration is infiltrated, silk cocoon is absorbed water, infiltration water temperature is 45~55 DEG C, time of penetration is 5~10 minutes, and for the control of the pH value of water 7~8, vacuum is 0.07~0.1Mpa.
S3. filature:Automatic silk reeling machine, filature speed 180r~240r/min are selected during filature, croisure length control exists 10mm~12mm.
S4. refine:
(1) pre-process:The silk made using low temperature plasma to S4 carries out pre-treatment;
(2) just practice:Prepare and just practice liquid, by pretreated silk, be put into and just practice in liquid, bath raio 1:20~30, heating Keep first liquid temperature degree of practicing to be maintained at 35~45 DEG C, be stirred continuously 20~40min of processing;
(3) it is multiple to practice:Prepare and practice liquid again, the silk practiced at the beginning of passing through is put into multiple experienced liquid, opens ultrasonic wave, ultrasonic frequency It is dehydrated after 20~60KHz, 20~30min of ultrasonication;
(4) bleach:Bleaching liquid is prepared, the silk Jing Guo dewater treatment is subjected to bleaching, treatment temperature is 60~80 DEG C, the time is 5~30min;
(5) clean:Cleaned with the water that temperature is 35~50 DEG C, be then dehydrated.
S5. it is expanded:Obtained silk in step S4 is put into the expanded agent solution of silk, vacuum be 0.91~ 0.95Mpa, temperature are 5~15min of silk of cryogenic vacuum infiltration processing dehydration at 20~25 DEG C, then place 6~10h;Will Silk after cryogenic vacuum infiltration processing immerses in the expanded agent solution of silk and adjusts pH value to 6~8.5, boil 5~ 10min, carry out expanding treatment.
S6. wash:Washed using ultrasound, Xi Sandao:First of washing is high temperature bath, 85~90 DEG C of temperature, the time 5~ 15min;Second washing is middle tepidarium, 50~60 DEG C of temperature, time 10min;3rd washing is room-temperature water bath, 5~ 10min。
S7. it is flame-retardant modified:Silk and treatment fluid after step S6 is washed is according to bath raio 1: 20~30, in 80-95 DEG C of temperature Under degree, immersion reaction treatment is taken out after 2~5 hours, then washs 2~5 dehydrations with deionized water;The treatment fluid includes tungsten Sour 3~5g of sodium, 2~5g of potassium fluotitanate, 3~8g of tartaric acid and deionized water 1000ml.
S8. dry:Silk after step S7 cleaning and dewaterings is dried, regain is controlled 8~10%.
As a kind of preferable scheme, in step S4, described low-temperature plasma pre-treatment, the gas used for nitrogen, Vacuum is 3~5Pa, and pressure is 100~150Pa, and processing time is 10~20min.
As a kind of preferable scheme, in step S4, the liquid of just practicing includes by mass percentage:0.2%~0.3% Sodium metasilicate, 0.2%~0.4% hydrogen peroxide, surplus are water.
As a kind of preferable scheme, in step S4, the liquid of practicing again is by mass percentage including 0.1%~0.2% Na2CO3, 0.3%~0.5% sodium metasilicate, 0.4%~0.6% AEO and 0.1%~0.15% alkane Base phenol ethylene oxide condensates, surplus are water.
As a kind of preferable scheme, in step S4, the bleaching liquid includes 0.5~2g/L of thiourea dioxide and sodium hydrosulfite 0.1~0.4g/L.
As a kind of preferable scheme, in step S5, the expanded agent solution of silk includes according to parts by weight:Na2SiO3 20~40 parts, 5~10 parts of ester based quaternary ammonium salt, 0.3~0.8 part of silicane-modified polyurethane, 0.1~0.5 part of soap powder, polyacrylamide 0.1~0.5 part, 0.1~0.5 part of calcium lignosulfonate, 0.1~0.5 part of citric acid, 0.1~0.5 part of xanthans, quinoxyfen 0.1 ~0.5 part, 500 parts of deionized water.
Due to using above-mentioned technical proposal, the invention has the advantages that:
1. the manufacture craft of the mulberry silk of the present invention, after silk cocoon is refrigerated, keeps the freshness of silkworm chrysalis, by fresh silk cocoon Directly by can directly be reeled off raw silk from cocoons after vacuum infiltration, reduce drying, cocoon cooking link, saving of labor, time saving, energy-conservation.And by mulberry Fresh silkworm cocoon processes mulberry silk, remaining fresh pupa, it is empty can to create bigger profit as food and the quality raw materials of biological products Between.And traditional silk production method, by silk cocoon by drying, and after silk cocoon is by drying, the silkworm chrysalis inside silk cocoon also can Die in succession.Also need to cocoon cooking, it is not only time-consuming, take a lot of work, and consume the energy.
2. the manufacture craft of the mulberry silk of the present invention, before refining, is first pre-processed, pre- using low temperature plasma It processing, can be broken silk gum macromolecular chain, silk gum layer cracking is loose, so as to accelerate just to practice liquid in later process and practice liquid again Infiltration and effect, reduce action time.Refining process using just practice and again practice by the way of, progressively degumming, degumming more thoroughly, And mulberry silk is damaged smaller.
3. the manufacture craft of the mulberry silk of the present invention, by carrying out expanding treatment using swelling agent to silk, silkworm can be increased Silk fiber bulkiness, high resiliency, flexibility, not haircuts, entanglement between silk fiber can be effectively prevented, improve the practicality of mulberry silk. By flame retardant treatment, silk inflaming retarding is assigned.As a result of appropriate crosslinking agent respectively with the amido in the macromolecular of silk Reacted with fire retardant so that fire retardant is stably connected with the macromolecular of down feathers, can have flame-retardant silk water-fastness With permanent fire retardant performance, and the fluffy degree and warmth retention property of silk are not influenceed.
4. the manufacture craft of the mulberry silk of the present invention, reduces fresh cocoon technological operation difficulty, is advantageous to energy-conserving and environment-protective, and Extremely advantageous condition is provided for the recovery and purification of subsequent production;The processing method of the present invention is simple, easily operated, and can The energy is saved, is had a good application prospect.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
Embodiment 1
A kind of manufacture craft of mulberry silk, comprises the following steps:
S1. refrigerate:The fresh silkworm cocoon freezing of butterfly is not changed pupa but, cryogenic temperature is controlled at -20~-15 DEG C, soon Speed kills fresh silkworm cocoon, and then temperature is slowly warming up to -10~-5 DEG C of preservations, keeps the freshness of fresh silkworm cocoon.
S2. vacuum infiltration:The method of silk cocoon vacuum infiltration after refrigeration is infiltrated, silk cocoon is absorbed water, infiltration water temperature is 45~55 DEG C, time of penetration is 10 minutes, and the control of the pH value of water is 7, vacuum 0.08Mpa.
S3. filature:Automatic silk reeling machine, filature speed 180r~240r/min are selected during filature, croisure length control exists 10mm~12mm.
S4. refine:
(1) pre-process:The silk made using low temperature plasma to S4 carries out pre-treatment;Before described low-temperature plasma Processing, the gas used is nitrogen, vacuum 5Pa, pressure 100Pa, processing time 15min.
(2) just practice:Prepare and just practice liquid, by pretreated silk, be put into and just practice in liquid, bath raio 1:20, heating is kept Just practice liquid temperature degree and be maintained at 35~40 DEG C, be stirred continuously processing 30min;The liquid of just practicing includes by mass percentage:0.2% Sodium metasilicate, 0.3% hydrogen peroxide, surplus are water.
(3) it is multiple to practice:Prepare and practice liquid again, the silk practiced at the beginning of passing through is put into multiple experienced liquid, opens ultrasonic wave, ultrasonic frequency It is dehydrated after 50KHz, ultrasonication 25min;It is described to practice the Na that liquid includes 0.2% by mass percentage again2CO3, 0.3% silicon Sour sodium, 0.5% AEO and 0.15% alkyl phenol ethylene oxide condensation product, surplus are water.
(4) bleach:Bleaching liquid is prepared, the silk Jing Guo dewater treatment is subjected to bleaching, treatment temperature is 65~70 DEG C, time 20min;The bleaching liquid includes thiourea dioxide 1g/L and sodium hydrosulfite 0.2g/L.
(5) clean:Cleaned with the water that temperature is 40~45 DEG C, be then dehydrated.
S5. it is expanded:Obtained silk in step S4 is put into the expanded agent solution of silk, is 0.95Mpa in vacuum, temperature The silk 10min for cryogenic vacuum infiltration processing dehydration at 20~25 DEG C is spent, then places 8h;After cryogenic vacuum infiltration is handled Silk immerse in the expanded agent solution of silk and adjust pH value to 7, boil 10min, carry out expanding treatment.
The expanded agent solution of silk includes according to parts by weight:Na2SiO330It is part, 8 parts of ester based quaternary ammonium salt, silane-modified poly- 0.5 part of urethane, 0.3 part of soap powder, 0.2 part of polyacrylamide, 0.3 part of calcium lignosulfonate, 0.3 part of citric acid, xanthans 0.2 Part, 0.3 part of quinoxyfen, 500 parts of deionized water.
S6. wash:Washed using ultrasound, Xi Sandao:First of washing is high temperature bath, 85~90 DEG C of temperature, the time 10min;Second washing is middle tepidarium, 50~60 DEG C of temperature, time 10min;3rd washing is room-temperature water bath, 10min.
S7. it is flame-retardant modified:Silk and treatment fluid after step S6 is washed are according to bath raio 1: 20, at a temperature of 90-95 DEG C, Immersion reaction treatment is taken out after 4 hours, then washs 3 dehydrations with deionized water;The treatment fluid includes sodium tungstate 3g, fluorine titanium Sour potassium 3g, tartaric acid 5g and deionized water 1000ml.
S8. dry:Silk after step S7 is dehydrated is dried, and regain is controlled 8%.
Embodiment 2
A kind of manufacture craft of mulberry silk, comprises the following steps:
S1. refrigerate:The fresh silkworm cocoon freezing of butterfly is not changed pupa but, cryogenic temperature is controlled at -20~-15 DEG C, soon Speed kills fresh silkworm cocoon, and then temperature is slowly warming up to -10~-5 DEG C of preservations, keeps the freshness of fresh silkworm cocoon.
S2. vacuum infiltration:The method of silk cocoon vacuum infiltration after refrigeration is infiltrated, silk cocoon is absorbed water, infiltration water temperature is 45~55 DEG C, time of penetration is 8 clocks, and the pH value control of water is 7~8, vacuum 0.95Mpa.
S3. filature:Automatic silk reeling machine, filature speed 180r~240r/min are selected during filature, croisure length control exists 10mm~12mm.
S4. refine:
(1) pre-process:The silk made using low temperature plasma to S4 carries out pre-treatment;Before described low-temperature plasma Processing, the gas used is nitrogen, vacuum 5Pa, pressure 120Pa, processing time 10min.
(2) just practice:Prepare and just practice liquid, by pretreated silk, be put into and just practice in liquid, bath raio 1:30, heating is kept Just practice liquid temperature degree and be maintained at 35~45 DEG C, be stirred continuously processing 40min;The liquid of just practicing includes by mass percentage:0.3% Sodium metasilicate, 0.2% hydrogen peroxide, surplus are water.
(3) it is multiple to practice:Prepare and practice liquid again, the silk practiced at the beginning of passing through is put into multiple experienced liquid, opens ultrasonic wave, ultrasonic frequency It is dehydrated after 50KHz, 20~30min of ultrasonication;It is described to practice the Na that liquid includes 0.1% by mass percentage again2CO3, 0.3% Sodium metasilicate, 0.6% AEO and 0.15% alkyl phenol ethylene oxide condensation product, surplus be water.
(4) bleach:Bleaching liquid to be prepared, the silk Jing Guo dewater treatment is subjected to bleaching, treatment temperature is 70 DEG C, when Between be 15min;The bleaching liquid includes thiourea dioxide 1g/L and sodium hydrosulfite 0.4g/L.
(5) clean:Cleaned with the water that temperature is 45~50 DEG C, be then dehydrated.
S5. it is expanded:
Obtained silk in step S4 is put into the expanded agent solution of silk, is 0.93Mpa in vacuum, temperature is 20 DEG C The silk 15min of lower cryogenic vacuum infiltration processing dehydration, then places 10h;Silk after cryogenic vacuum infiltration is handled immerses In the expanded agent solution of silk and pH value is adjusted to 8, is boiled 6min, is carried out expanding treatment.
The expanded agent solution of silk includes according to parts by weight:Na2SiO330 parts, it is 5 parts of ester based quaternary ammonium salt, silane-modified poly- 0.3 part of urethane, 0.5 part of soap powder, 0.1 part of polyacrylamide, 0.5 part of calcium lignosulfonate, 0.1 part of citric acid, xanthans 0.5 Part, 0.2 part of quinoxyfen, 500 parts of deionized water.
S6. wash:Washed using ultrasound, Xi Sandao:First of washing is high temperature bath, 85~90 DEG C of temperature, the time 5min;Second washing is middle tepidarium, 50~60 DEG C of temperature, time 10min;3rd washing is room-temperature water bath, 10min.
S7. it is flame-retardant modified:Silk and treatment fluid after step S6 is washed are according to bath raio 1: 30, at a temperature of 85-90 DEG C, Immersion reaction treatment is taken out after 5 hours, then washs 4 dehydrations with deionized water;The treatment fluid includes sodium tungstate 5g, fluorine titanium Sour potassium 3g, tartaric acid 5g and deionized water 1000ml.
S8. dry:Silk after step S7 is dehydrated is dried, and regain is controlled 9%.
Described above is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair Bright patent claim, the equal change completed or modification change under the technical concept suggested by all present invention, all should belong to Cover the scope of the claims in the present invention.

Claims (6)

1. a kind of manufacture craft of mulberry silk, it is characterised in that comprise the following steps:
S1. refrigerate:The fresh silkworm cocoon freezing of butterfly is not changed pupa but, cryogenic temperature is controlled at -20~-15 DEG C, quickly killed Dead fresh silkworm cocoon, then temperature be slowly warming up to -10~-5 DEG C of preservations, keep the freshness of fresh silkworm cocoon;
S2. vacuum infiltration:The method of silk cocoon vacuum infiltration after refrigeration is infiltrated, silk cocoon is absorbed water, infiltration water temperature is 45~ 55 DEG C, time of penetration is 5~10 minutes, and for the control of the pH value of water 7~8, vacuum is 0.07~0.1Mpa;
S3. filature:Select automatic silk reeling machine during filature, filature speed 180r~240r/min, croisure length control 10mm~ 12mm;
S4. refine:
(1) pre-process:The silk made using low temperature plasma to S4 carries out pre-treatment;
(2) just practice:Prepare and just practice liquid, by pretreated silk, be put into and just practice in liquid, bath raio 1:20~30, heating is kept Just practice liquid temperature degree and be maintained at 35~45 DEG C, be stirred continuously 20~40min of processing;
(3) it is multiple to practice:To prepare and practice liquid again, the silk practiced at the beginning of passing through is put into multiple experienced liquid, unlatching ultrasonic wave, ultrasonic frequency 20~ It is dehydrated after 60KHz, 20~30min of ultrasonication;
(4) bleach:Bleaching liquid to be prepared, the silk Jing Guo dewater treatment is subjected to bleaching, treatment temperature is 60~80 DEG C, when Between be 5~30min;
(5) clean:Cleaned with the water that temperature is 35~50 DEG C, be then dehydrated;
S5. it is expanded:Obtained silk in step S4 is put into the expanded agent solution of silk, is 0.91~0.95Mpa in vacuum, Temperature is 5~15min of silk of cryogenic vacuum infiltration processing dehydration at 20~25 DEG C, then places 6~10h;By cryogenic vacuum Silk after infiltration processing immerses in the expanded agent solution of silk and adjusts pH value to 6~8.5, boils 5~10min, carries out Expanding treatment;
S6. wash:Washed using ultrasound, Xi Sandao:First of washing is high temperature bath, 85~90 DEG C of temperature, the time 5~ 15min;Second washing is middle tepidarium, 50~60 DEG C of temperature, time 10min;3rd washing is room-temperature water bath, 5~ 10min;
S7. it is flame-retardant modified:Silk and treatment fluid after step S6 is washed are according to bath raio 1: 20~30, at a temperature of 80-95 DEG C, Immersion reaction treatment is taken out after 2~5 hours, then washs 2~5 dehydrations with deionized water;The treatment fluid includes sodium tungstate 3 ~5g, 2~5g of potassium fluotitanate, 3~8g of tartaric acid and deionized water 1000ml;
S8. dry:Silk after step S7 cleaning and dewaterings is dried, regain is controlled 8~10%.
2. the manufacture craft of mulberry silk according to claim 1, it is characterised in that in step S4, described low temperature etc. from Sub- pre-treatment, for the gas used for nitrogen, vacuum is 3~5Pa, and pressure is 100~150Pa, processing time is 10~ 20min。
3. the manufacture craft of mulberry silk according to claim 1, it is characterised in that in step S4, the liquid of just practicing presses matter Amount percentage includes:0.2%~0.3% sodium metasilicate, 0.2%~0.4% hydrogen peroxide, surplus are water.
4. the manufacture craft of mulberry silk according to claim 1, it is characterised in that in step S4, the liquid of practicing again presses matter Amount percentage includes 0.1%~0.2% Na2CO3, 0.3%~0.5% sodium metasilicate, 0.4%~0.6% fatty alcohol polyoxy Vinethene and 0.1%~0.15% alkyl phenol ethylene oxide condensation product, surplus are water.
5. the manufacture craft of mulberry silk according to claim 1, it is characterised in that in step S4, the bleaching liquid includes 0.1~0.4g/L of 0.5~2g/L of thiourea dioxide and sodium hydrosulfite.
6. the manufacture craft of mulberry silk according to claim 1, it is characterised in that in step S5, the silk swelling agent Solution includes according to parts by weight:Na2SiO320~40 parts, 5~10 parts of ester based quaternary ammonium salt, silicane-modified polyurethane 0.3~0.8 Part, 0.1~0.5 part of soap powder, 0.1~0.5 part of polyacrylamide, 0.1~0.5 part of calcium lignosulfonate, citric acid 0.1~0.5 Part, 0.1~0.5 part of xanthans, 0.1~0.5 part of quinoxyfen, 500 parts of deionized water.
CN201710904004.6A 2017-09-29 2017-09-29 A kind of manufacture craft of mulberry silk Pending CN107699958A (en)

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CN111394804A (en) * 2020-03-25 2020-07-10 杭州金利丝业有限公司 Manufacturing method of flexible breathable mulberry silk
CN115137869A (en) * 2022-06-08 2022-10-04 苏州大学 Reinforced and toughened silk suture and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN109811560A (en) * 2019-01-26 2019-05-28 桐乡市钜汪家纺有限公司 A kind of production technology of seven color silk cottons
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Application publication date: 20180216